HCID 86640142, compound → HCID 59245587, compound
Reaction equation
[CH2:1]([O:3][Si:4]([C:11]1[CH2:14][CH2:13][C:12]=1[Si:15]([O:22][CH2:23][CH3:24])([O:19][CH2:20][CH3:21])[O:16][CH2:17][CH3:18])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2]>[Cu]Cl>[CH2:17]([O:16][Si:15]([O:22][CH2:23][CH3:24])([O:19][CH2:20][CH3:21])[CH:12]1[CH2:13][CH2:14][CH:11]1[Si:4]([O:5][CH2:6][CH3:7])([O:3][CH2:1][CH3:2])[O:8][CH2:9][CH3:10])[CH3:18]Participants
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
1,2-Bis(tri-ethoxysilyl)acetylene represented by formula (A) was mixed with 1.2 mol equivalent of zirconocene diethyl, and the mixture was stirred at room temperature for one hr. Subsequently, 1.2 mol equivalent of iodine was mixed thereinto, and the mixture was stirred at 0° C. for 2 hr. Finally, 1.2 mol equivalent of copper(I) chloride was mixed thereinto, and the mixture was stirred at room temperature for 6 hr. Thus, the reactions were successively performed. Thereafter, the reaction solution was filtered to remove salts. The filtrate was then concentrated under the reduced pressure, and the concentrate was purified by column chromatography on alumina to give 1,2-bis(tri-ethoxysilyl)cyclobutene as a substituted position isomer mixture at a yield of 60%. In the reaction with copper(I) chloride, the yield of bis(tri-ethoxysilyl)cyclobutene when 0.1 mol equivalent of copper(I) chloride was mixed followed by stirring at room temperature for 24 hr was identical to the yield of bis(tri-ethoxysilyl)cyclobutene when 0.1 mol equivalent of copper(I) chloride was mixed followed by stirring at 50° C. for 6 hr. Subsequently, a hydrogenation reaction is performed to give 1,2-bis(tri-ethoxysilyl)cyclobutane (I-1).
Workup
- additionwas mixed
- stirringby stirring at 50° C. for 6 hr
- customSubsequently, a hydrogenation reaction
Sources & evidence
- ORD record
- ord-44272967fefb4a2e90d38626534aa654
- Source dataset
- uspto-grants-2011_08
- Patent number
- US07999356B2
Reaction notes
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